ATE538069T1 - METHOD FOR THE CONTINUOUS PRODUCTION OF POLYCRYSTALLINE HIGH-PURITY SILICON GRANULES - Google Patents

METHOD FOR THE CONTINUOUS PRODUCTION OF POLYCRYSTALLINE HIGH-PURITY SILICON GRANULES

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Publication number
ATE538069T1
ATE538069T1 AT08155254T AT08155254T ATE538069T1 AT E538069 T1 ATE538069 T1 AT E538069T1 AT 08155254 T AT08155254 T AT 08155254T AT 08155254 T AT08155254 T AT 08155254T AT E538069 T1 ATE538069 T1 AT E538069T1
Authority
AT
Austria
Prior art keywords
gas
silicon
bed
fluidized
reaction
Prior art date
Application number
AT08155254T
Other languages
German (de)
Inventor
Dieter Weidhaus
Rainer Hauswirth
Harald Hertlein
Original Assignee
Wacker Chemie Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wacker Chemie Ag filed Critical Wacker Chemie Ag
Application granted granted Critical
Publication of ATE538069T1 publication Critical patent/ATE538069T1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Silicon Compounds (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The method for producing highly pure polycrystalline silicon granulates by depositing a reaction gas of silicon granulates in a fluidized-bed reactor, comprises slightly fluidizing a lower zone (5) of a reactor chamber of a reactor by introducing a silicon-free gas by individual nozzles in the silicon granulates, directly connecting an upper zone of the reactor chamber with the lower zone, heating the zones over its external limiting wall, and injecting a silicon-containing reaction gas into the formed reaction zone by nozzles with high-speed than vertically arranged gas jet. The method for producing highly pure polycrystalline silicon granulates by depositing a reaction gas of silicon granulates in a fluidized-bed reactor, comprises slightly fluidizing a lower zone (5) of a reactor chamber of a reactor by introducing a silicon-free gas by individual nozzles in the silicon granulates, directly connecting an upper zone of the reactor chamber with the lower zone, heating the zones over its external limiting wall, and injecting a silicon-containing reaction gas into the formed reaction zone by nozzles with high-speed than vertically arranged gas jet. The local reaction gas jets surrounded by blow-forming fluidized-bed (2) are formed itself above the nozzles. The silicon-containing gas (11) decomposes itself at the particles surfaces within the fluidized-bed and leads for particle growth. The reaction gas is reacted almost up to the chemical equilibrium conversion before it reaches into the fluidized-bed wall or the fluidized-bed surface. The height of the lower zone is laid out so that no reaction gas flows back up to the nozzles for the dilution gas (12) for the fluidization of the lower zone and is blocked by the wall separator. The height of the lower zone is 50-300 mm. The dilution gas is supplied in a quantity to the nozzles. The gas speed in the lower zone is 1.2 to 2.3-times of the releasing gas speed. The maximum exhaust speed of the dilution gas from the nozzles is 20-200 m/s. The silicon-containing gases are used as reaction gas to the general compound of silicon hydrochloride (SiH xCl y) or mixtures of these gases are used as dilution gas with silicon-free gases. The mole fraction of trichlorosilane in the reaction gas is 0.2-0.8. The average mole fraction and the dilution gas from the lower zone over the entire reactor cross section is 0.15-0.4. The local gas speeds of the gases and/or the gas mixtures at the exit of the nozzle system are 1-140 m/s. The average gas speed in the reaction zone is 2-8 times of releasing gas speed. The minimum distance of the nozzles is selected to each other in such a way that the ratio of the nozzle distance to nozzle diameter is larger than 7.5. The exit speed at the annular nozzle is smaller than the exit speed at the central nozzle. The speed at the annular nozzle (V a n n u l a r n o z z l e) is 0.4-0.8 V c e n t r a l n o z z l e. The retention time of the gas in the upper zone of the fluidized-bed is 0.1-10 seconds. The bed temperature of the fluidized-bed is 890-1400[deg] C. The reactor pressure is positive pressure of 0-7 bar. The operation of the fluidized-bed has a stationary particle size distribution. The particles are 150-7000 mu m larger and the sauter diameter of the distribution is 850-1500 mu m. On-line exhaust gas analytics are used for the determination of the reaction conversion. The addition of the germ particles and the product distraction are steered in combination with the collection of the quantities on supplied reaction- and dilution gas and a computer model for particle population, so that the desired particle size distribution in the reactor and the quantity of granulates in the fluidized-bed are stable and stationarily kept over a long period of time. The undersize portion at the particles of less than 150 mu m lies under 0.1 mass percent, without necessary of additional classification step. The deposited polysilicon granulates have an expressed spherical form having sphericity value of 0.85 to 1 [-].
AT08155254T 2007-05-04 2008-04-28 METHOD FOR THE CONTINUOUS PRODUCTION OF POLYCRYSTALLINE HIGH-PURITY SILICON GRANULES ATE538069T1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102007021003A DE102007021003A1 (en) 2007-05-04 2007-05-04 Process for the continuous production of polycrystalline high-purity silicon granules

Publications (1)

Publication Number Publication Date
ATE538069T1 true ATE538069T1 (en) 2012-01-15

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Country Status (8)

Country Link
US (1) US8722141B2 (en)
EP (1) EP1990314B1 (en)
JP (1) JP4971240B2 (en)
KR (1) KR101026815B1 (en)
CN (1) CN101298329B (en)
AT (1) ATE538069T1 (en)
DE (1) DE102007021003A1 (en)
ES (1) ES2376695T3 (en)

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Also Published As

Publication number Publication date
CN101298329B (en) 2012-01-04
DE102007021003A1 (en) 2008-11-06
EP1990314B1 (en) 2011-12-21
ES2376695T3 (en) 2012-03-16
JP2008273831A (en) 2008-11-13
KR20080098322A (en) 2008-11-07
US8722141B2 (en) 2014-05-13
EP1990314A2 (en) 2008-11-12
US20080299291A1 (en) 2008-12-04
JP4971240B2 (en) 2012-07-11
EP1990314A3 (en) 2009-08-12
CN101298329A (en) 2008-11-05
KR101026815B1 (en) 2011-04-04

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